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Ammonium Hydroxide → 2-(3-Mercapto-1-oxopropyl)-5-oxo-3-pyrazolidinecarboxylic acid

HRID 27261
ノート
印刷プレビュー

反応式

HRID 27261 の反応式
C([S:4][CH2:5][CH2:6][C:7]([N:9]1[CH:13]([C:14]([OH:16])=[O:15])[CH2:12][C:11](=[O:17])[NH:10]1)=[O:8])(=O)C.[OH-].[NH4+]>>[SH:4][CH2:5][CH2:6][C:7]([N:9]1[CH:13]([C:14]([OH:16])=[O:15])[CH2:12][C:11](=[O:17])[NH:10]1)=[O:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 14923Ammonium HydroxideHCID 23344444HCID 23344444、化合物

生成物 1

HCID 233444412-(3-Mercapto-1-oxopropyl)-5-oxo-3-pyrazolidinecarboxylic acid収率 44.7%

実験手順

DL-2-[3-(Acetylthio)-1-oxopropyl]-5-oxo-3-pyrazolidinecarboxylic acid (1.2 g) is treated in an argon atmosphere with 8 ml of a cold solution of 6.5 N ammonium hydroxide. After one hour at room temperature, the solution is extracted with ethyl acetate and treated with concentrated hydrochloric acid to pH 2. The water soluble product is extracted with five 20 ml portions of ethyl acetate. The combined extracts are dried over magnesium sulfate and evaporated to an oil which gradually solidifies. This material is dried in vacuo at 100° C. for 1 hour yielding 0.45 g of the title compound, melting point 140°-142° C.

後処理

  1. extractionthe solution is extracted with ethyl acetate
  2. addition
treated with concentrated hydrochloric acid to pH 2
  • extractionThe water soluble product is extracted with five 20 ml portions of ethyl acetate
  • dry with materialThe combined extracts are dried over magnesium sulfate
  • customevaporated to an oil which
  • customThis material is dried in vacuo at 100° C. for 1 hour
  • 出典と根拠

    ORDレコード
    ord-39f6373776314ee2a372f4309ef8097e
    出典データセット
    uspto-grants-1980_09
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US04220791

    反応ノート

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